Ferroelectric Phase Content in 7 nm Hf (1- x ) Zr x O 2 Thin Films Determined by X-Ray-Based Methods
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To study nanostructures on substrates, surface-sensitive reflection-geometry scattering techniques such as grazing incident small angle X-ray scattering are commonly used to yield an averaged statistical structural information of the surface sample. Grazing incidence geometry can probe the absolute three-dimensional structural morphology of the sample if a highly coherent beam is used. Coherent surface scattering imaging (CSSI) is a powerful yet non-invasive technique similar to coherent X-ray diffractive imaging (CDI) but performed at small angles and grazing-incidence reflection geometry. A challenge with CSSI is that conventional CDI reconstruction techniques cannot be directly applied to CSSI because the Fourier-transform-based forward models cannot reproduce the dynamical scattering phenomenon near the critical angle of total external reflection of the substrate-supported samples. To overcome this challenge, we have developed a multislice forward model which can successfully simulate the dynamical or multi-beam scattering generated from surface structures and the underlying substrate. The forward model is also demonstrated to be able to reconstruct an elongated 3D pattern from a single shot scattering image in the CSSI geometry through fast-performing CUDA-assisted PyTorch optimization with automatic differentiation.
Increased understanding of the effects of acoustic treatment on the propagation of sound through commercial aircraft engine nacelles is a requirement for more efficient liner design. To this end, one of NASA s goals is to further the development of duct propagation and impedance reduction codes. A number of these codes have been developed over the last three decades. These codes are typically divided into two categories: (1) codes that use the measured complex acoustic pressure field to reduce the acoustic impedance of treatment that is positioned along the wall of the duct, and (2) codes that use the acoustic impedance of the treatment as input and compute the sound field throughout the duct. Clearly, the value of these codes is dependent upon the quality of the data used for their validation. Over the past two decades, data acquired in the NASA Langley Research Center Grazing Incidence Tube have been used by a number of researchers for comparison with their propagation codes. Many of these comparisons have been based upon Grazing Incidence Tube tests that were conducted to study specific liner technology components, and were incomplete for general propagation code validation. Thus, the objective of the current investigation is to provide a quality data set that can be used as a benchmark for evaluation of duct propagation and impedance reduction codes. In order to achieve this objective, two parallel efforts have been undertaken. The first of these is the development of an enhanced impedance eduction code that uses data acquired in the Grazing Incidence Tube. This enhancement is intended to place the benchmark data on as firm a foundation as possible. The second key effort is the acquisition of a comprehensive set of data selected to allow propagation code evaluations over a range of test conditions.
NASA's Marshall Space Flight Center (MSFC) engages in research, development, design, fabrication, coating, assembly, and testing of grazing-incidence optics (primarily) for x-ray telescope systems. Over the past two decades, MSFC has refined processes for electroformed-nickel replication of grazing-incidence optics, in order to produce high-strength, thin-walled, full-cylinder x-ray mirrors. In recent years, MSFC has used this technology to fabricate numerous x-ray mirror assemblies for several flight (balloon, rocket, and satellite) programs. Additionally, MSFC has demonstrated the suitability of this technology for ground-based laboratory applications-namely, x-ray microscopes and cold-neutron microscopes and concentrators. This mature technology enables the production, at moderately low cost, of reasonably lightweight x-ray telescopes with good (15-30 arcsecond) angular resolution. However, achieving arcsecond imaging for a lightweight x-ray telescope likely requires development of other technologies. Accordingly, MSFC is conducting a multi-faceted research program toward enabling cost-effective production of lightweight high-resolution x-ray mirror assemblies. Relevant research topics currently under investigation include differential deposition for post-fabrication figure correction, in-situ monitoring and control of coating stress, and direct fabrication of thin-walled full-cylinder grazing-incidence mirrors.
NASA's Marshall Space Flight Center (MSFC) engages in research, development, design, fabrication, coating, assembly, and testing of grazing-incidence optics (primarily) for x-ray telescope systems. Over the past two decades, MSFC has refined processes for electroformed-nickel replication of grazing-incidence optics, in order to produce high-strength, thin-walled, full-cylinder x-ray mirrors. In recent years, MSFC has used this technology to fabricate numerous x-ray mirror assemblies for several flight (balloon, rocket, and satellite) programs. Additionally, MSFC has demonstrated the suitability of this technology for ground-based laboratory applications-namely, x-ray microscopes and cold-neutron microscopes and concentrators. This mature technology enables the production, at moderately low cost, of reasonably lightweight x-ray telescopes with good (15-30 arcsecond) angular resolution. However, achieving arcsecond imaging for a lightweight x-ray telescope likely requires development of other technologies. Accordingly, MSFC is conducting a multi-faceted research program toward enabling cost-effective production of lightweight high-resolution x-ray mirror assemblies. Relevant research topics currently under investigation include differential deposition for post-fabrication figure correction, in-situ monitoring and control of coating stress, and direct fabrication of thin-walled full-cylinder grazing-incidence mirrors.
Focusing optics based on Wolter optical geometries developed for x-ray grazing incidence beams can be designed for neutron beams. Wolter optics are formed by grazing incidence reflections from two concentric conic sections (for example, a paraboloid and a hyperboloid). This has transformed observational X-ray astronomy by increasing the sensitivity by many orders of magnitude for research in astrophysics and cosmology. To increase the collection area, many reflecting mirrors of different diameters are nested with a common focal plane. These mirrors are fabricated using nickel-electroformed replication techniques. We apply these ideas to neutron focusing using nickel mirrors. We show an initial test of a conical mirror using a beam of cold neutrons. key words: electroformed nickel replication, focusing optics, grazing angle incidence, mirror reflection, neutron focusing, Wolter optics
Coherent X-ray imaging is an active field at synchrotron sources. The images rely on the available coherent flux over a limited field of view. At many synchrotron beamlines a double-crystal monochromator (DCM) is employed in a standard nondispersive arrangement. For coherent diffraction imaging it is advantageous to increase the available field of view by increasing the spatial coherence length (SCL) of a beam exiting such a DCM. Here, Talbot interferometry data together with ray-tracing simulations for a (+ − − +) four-reflection experimental arrangement are presented, wherein the first two reflections are in the DCM and the final fourth reflection is asymmetric at grazing exit. Analyses of the interferometry data combined with the simulations show that compared with the beam exiting the DCM a gain of 76% in the SCL was achieved, albeit with a factor of 20 reduction in flux density, which may not be a severe penalty at a synchrotron beamline. Previous efforts reported in the literature to increase the SCL that employed asymmetric crystal diffraction at grazing incidence are also discussed. A much reduced SCL is found presently in simulations wherein the same asymmetric crystal is set for grazing incidence instead of grazing exit. In addition, the present study is compared and contrasted with two other means of increasing the SCL. These are (i) focusing the beam onto an aperture to act as a secondary source, and (ii) allowing the beam to propagate in vacuum an additional distance along the beamline.
Sputter deposition is a versatile and industrially important deposition technique for thin films, with increasing demand for matching the characteristics of thin film materials to specific requirements. Additionally, the actual film properties are largely determined by sputtering parameters such as pressure conditions, temperature and power settings. By means of various X-ray diffraction and scattering techniques, it is shown that the characterization of film formation and growth is feasible in real time at synchrotron sources, thus adding an important dimension to the fundamental understanding of the evolution of thin film microstructure. In particular, grazing incidence small-angle X-ray scattering, grazing incidence X-ray powder diffraction and X-ray reflectometry are used in a complementary manner to study the influence of deposition temperature and substrate choice on the crystallization kinetics and growth of polycrystalline BaTiO 3 films.
The XUV spectroheliometer for the Solar Maximum Mission (SMM) is described. This instrument is a grazing-incidence polychromatic photoelectric spectrometer illuminated by a grazing-incidence telescope mirror. The wavelength range is 20-1336 A, the spectral resolution is between 0.1 and 0.3 A, and the spatial resolution is 4 arcsec. Simultaneous spectroheliograms in twelve spectral lines are obtained by rastering the instrument at variable rates. The scientific objectives and the mission operations concept are also described.
The self-assembly of block copolymers (BCPs) in thin films is governed by interfacial interactions (enthalpy) between the blocks and interfaces (at both the substrate and the surface). Advantage can also be taken of entropy to control the polymer orientation. Here, we synthesized a series of bottlebrush block copolymers (BBCPs), with deuterated polystyrene (DPS) as the core block and poly(solketal acrylate) (PSA) as the corona block, where the backbone length (N BB) and grafting densities (GDs) were varied. The hydrophobic PSA block was converted to a hydrophilic poly(glyceryl acrylate) (PGA) block by solid-state hydrolysis, bringing the BBCP from a disordered state into an ordered state with a lamellar microdomain morphology. The orientation of the morphology as a function of distance from the interfaces was systematically investigated by atomic force microscopy (AFM), interference microscopy, grazing-incidence small-angle X-ray scattering (GISAXS), and grazing-incidence small angle neutron scattering (GISANS). For N BB = 1 (diblock BCP), a mixed lamellar orientation was found. For N BB = 5 (star-like BBCP), a vertical orientation of the lamellar microdomains was found dominantly at the interfaces that propagated into the bulk of the film due to the entropic penalty associated with constraints on the junction points. Increasing the N BB to 50 (rod-like BBCP) and 100 (worm-like BBCP) yielded a random orientation, as the side chains became overcrowded when aligned in the same direction. By reducing the grafting density (GD) of a N BB = 50 BBCP from 100% to 75% and 50% by the incorporation of spacers into the backbone, the steric hindrance of side chains is reduced markedly, facilitating a vertical orientation of the lamellar microdomains. However, the vertical orientation becomes more random within the bulk of the thin film for different BBCP architectures. By modifying the substrate with a layer of PS, the preferential interactions between the core block of the BBCP and the interfaces induce a reconfiguration of the BBCP, drawing the core block out to contact substrate directly driven by enthalpy. Under these conditions, N BB = 5 showed a predominantly parallel orientation of the lamellar microdomains with the corona block minimizing contact with the substrate. Higher N BB values of 50 and 100 showed a more random orientation of the lamellar microdomains at different depths on the PS-modified substrate. Overall, thin-film morphology was regulated by tuning the configuration of the BBCP, varying the entropic contribution to the microdomain orientation.
A considerable amount of effort over the past year has been devoted to exploring ultra-lightweight optics for two specific NASA programs, the Next Generation Space Telescope (NGST), and the High Throughput X-ray Spectrometer (HTXS). Experimental investigations have been undertaken in a variety of materials including glass, composites, nickel, beryllium, Carbon Silicon Carbide, Reaction Bonded Silicon Carbide, Chemical Vapor Deposited Silicon Carbide, and silicon. Overall results of these investigations will be summarized, and specific details will be provided concerning the in-house development of ultra-lightweight nickel replication for both grazing incidence and normal incidence optics. This will include x-ray test results of the grazing incidence optic and cryogenic test results of the normal incidence optic. The status of two 1.5 meter diameter demonstration mirrors for NGST will also be presented. These two demonstrations are aimed at establishing the capability to manufacture and test mirrors that have an areal density of 15 kilograms per square meter.
The application of grazing-incidence total X-ray scattering (GITXS) for pair distribution function (PDF) analysis using >50 keV X-rays from synchrotron light sources has created new opportunities for structural characterization of supported thin films with high resolution. Compared with grazing-incidence wide-angle X-ray scattering, which is only useful for highly ordered materials, GITXS/PDFs expand such analysis to largely disordered or nanostructured materials by examining the atomic pair correlations dependent on the direction relative to the surface of the supporting substrate. A characterization of nanocrystalline In 2 O 3 -derived thin films is presented here with in-plane-isotropic and out-of-plane-anisotropic orientational ordering of the atomic structure, each synthesized using different techniques. The atomic orientations of such films are known to vary based on the synthetic conditions. Here, an azimuthal orientational analysis of these films using GITXS with a single incident angle is shown to resolve the markedly different orientations of the atomic structures with respect to the planar support and the different degrees of long-range order, and hence, the terminal surface chemistries. It is anticipated that orientational analysis of GITXS/PDF data will offer opportunities to extend structural analyses of thin films by providing a means to qualitatively determine the major atomic orientation within nanocrystalline and, eventually, non-crystalline films.
M-STAR is a next generation polarized neutron reflectometer with advanced capabilities. A new focusing guide concept is optimized for samples with dimensions down to a millimeter range. A proposed hybrid pulse-skipping chopper will enable experiments at constant geometry at one incident angle in a broad range of wavevector transfer Q up to 0.3 A –1 for specular, off-specular, and GISANS measurements. M-STAR will empower nanoscience and spintronics studies routinely on small samples (~2 × 2 mm 2 ) and of atomic-scale thickness using versatile experimental conditions of magnetic and/or electric fields, light, and temperature applied in situ to novel complex device-like nanosystems with multiple buried interfaces. M-STAR will enable improved grazing incidence diffraction measurements, as a surface-sensitive depth-resolved probe of, e.g., the out-of-plane component of atomic magnetic moments in ferromagnetic, antiferromagnetic, and more complex structures as well as in-plane atomic-scale structures inaccessible with contemporary diffractometry and reflectometry. New horizons will be opened by the development of an option to probe near-surface dynamics with inelastic grazing incidence scattering in the time-of-flight mode. These novel options in combination with ideally matched parameters of the second target station will place M-STAR in the world’s leading position for high resolution polarized reflectometry.
This paper reports the initial results of a test series to evaluate a method for determining the normal incidence impedance of a locally reacting acoustically absorbing liner, located on the lower wall of a duct in a grazing incidence, multi-modal, non-progressive acoustic wave environment without flow. This initial evaluation is accomplished by testing the methods' ability to converge to the known normal incidence impedance of a solid steel plate, and to the normal incidence impedance of an absorbing test specimen whose impedance was measured in a conventional normal incidence tube. The method is shown to converge to the normal incident impedance values and thus to be an adequate tool for determining the impedance of specimens in a grazing incidence, multi-modal, nonprogressive acoustic wave environment for a broad range of source frequencies.
The Solar-A satellite being prepared by the Institute for Sapce and Astronautical Sciences (ISAS) in Japan is dedicated to high energy observations of solar flares. The Soft X Ray Telescope (SXT) is being prepared to provide filtered images in the 2 to 60 A interval. The flight model is now undergoing tests in the 1000 foot tunnel at MSFC. Launch will be in September 1991. Earlier resolution and efficiency tests on the grazing incidence mirror have established its performance in soft x rays. The one-piece, two mirror grazing incidence telescope is supported in a strain free mount separated from the focal plane assembly by a carbon-epoxy metering tube whose windings and filler are chosen to minimize thermal and hygroscopic effects. The CCD detector images both the x ray and the concentric visible light aspect telescope. Optical filters provide images at 4308 and 4700 A. The SXT will be capable of producing over 8000 of the smallest partial frame images per day, or fewer but larger images, up to 1024 x 1024 pixel images. Image sequence with two or more of the five x ray analysis filters, with automatic exposure compensation to optimize the charge collection by the CCD detector, will be used to provide plasma diagnostics. Calculations using a differential emission measure code were used to optimize filter selection over the range of emission measure variations and to avoid redundancy, but the filters were chosen primarily to give ratios that are monotonic in plasma temperature.
High resolution soft X-ray imaging from the solar probe is justified in terms of the expected scientific returns which include the determination of the temperature and density structure of a coronal loop. The advantages of the grazing incidence telescope over the multiple pinhole camera are discussed. An instrument package is described which includes a grazing incidence mirror, a thermal prefilter, a three position filter wheel and a focal plane detector baselined as an 800 by 800 back-illuminated charge coupled device. The structural assembly together with the data processing equipment would draw heavily on the designs being developed for the Solar Polar Mission.
Both scattering and figure errors in grazing incidence optics are larger in the plane of incidence than out-of-plane by a factor equal to 1/sin theta, where theta is the graze angle. When the full annular aperture of a grazing incidence telescope is stopped down, the point spread function becomes highly elliptical with a width as much as sin theta times narrower than the full image. In practice, this means that improvements in resolution of up to 100 times can be achieved, and effective resolution can approach the diffraction limit. Laboratory data demonstrating the effect are presented.
In the case of neutrons the refractive index is slightly less than unity for most elements and their isotopes. Consequently, thermal and cold neutrons can be reflected from smooth surfaces at grazing-incidence angles. Hence, the optical technologies developed for x-ray astronomy can be applied for neutron focusing. The focusing capabilities of grazing incidence neutron imaging optics have been successfully demonstrated using nickel mirrors. The mirrors were fabricated using an electroformed nickel replication process at Marshall Space Flight Center. Results of the neutron optics experiments will be presented. Challenges of the neutron imaging optics as well as possible applications of the optics will be discussed.